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1-Amino-2-propanol → HCID 13881295, 화합물

HRID 231580
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HRID 231580 반응식
Cl[S:2]([C:5]1[CH:14]=[CH:13][CH:12]=[C:11]([N+:15]([O-:17])=[O:16])[C:6]=1[C:7]([O:9][CH3:10])=[O:8])(=[O:4])=[O:3].[NH2:18][CH2:19][CH:20]([OH:22])[CH3:21].Cl>C1COCC1>[OH:22][CH:20]([CH3:21])[CH2:19][NH:18][S:2]([C:5]1[CH:14]=[CH:13][CH:12]=[C:11]([N+:15]([O-:17])=[O:16])[C:6]=1[C:7]([O:9][CH3:10])=[O:8])(=[O:4])=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 41-Amino-2-propanolHCID 313Hydrochloric AcidHCID 13670189Methyl 2-(chlorosulfonyl)-6-nitrobenzoate

생성물 1

HCID 13881295HCID 13881295, 화합물수율 63.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of methyl 2-chlorosulfonyl-6-nitrobenzoate (2.80g, 10 mmol) in 100 ml of THF was cooled in an ice-bath and stirred while a solution of 1-amino-2-propanol (1.65g, 22 mmol) in 10 ml of THF was added dropwise over a period of 50 minutes. After stirring an additional 30 minutes in the ice-bath, the reaction mixture was acidified by the addition of 3 ml of 1.2N HCl. The THF was evaporated under reduced pressure and the residue taken up in 100 ml of ethyl acetate. After extracting with 4×20 ml of saturated NaCl solution, the ethyl acetate solution was dried over Na2SO4 and the solvent evaporated. The residue was crystallized from a mixture of ethyl acetate and hexane to give 2.02g (63.5%) of yellow crystalline product, m.p., 93.5-95°.

후처리

  1. additionwas added dropwise over a period of 50 minutes
  2. customThe THF was evaporated under reduced pressure
  3. extractionAfter extracting with 4×20 ml of saturated NaCl solution
  4. dry with materialthe ethyl acetate solution was dried over Na2SO4
  5. customthe solvent evaporated
  6. customThe residue was crystallized from a mixture of ethyl acetate and hexane

출처 및 근거

ORD 기록
ord-3eb88ee2dd034ef5a20228993ed08d0b
출처 데이터셋
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04847294

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